CN1782891A - 调色剂组合物 - Google Patents
调色剂组合物 Download PDFInfo
- Publication number
- CN1782891A CN1782891A CN200510128939.7A CN200510128939A CN1782891A CN 1782891 A CN1782891 A CN 1782891A CN 200510128939 A CN200510128939 A CN 200510128939A CN 1782891 A CN1782891 A CN 1782891A
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- CN
- China
- Prior art keywords
- toner
- colorant
- wax
- latex
- resin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
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Classifications
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
- G03G9/00—Developers
- G03G9/08—Developers with toner particles
- G03G9/087—Binders for toner particles
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Abstract
描述了包括基本没有交联的树脂;交联的树脂;蜡;和导电着色剂的调色剂组合物。
Description
技术领域
本公开内容涉及调色剂组合物,并更特别地涉及特别适用于高速打印机的乳液聚集黑色调色剂组合物,并进一步更特别地涉及具有优化的炭黑颜料含量用于改进图像质量以及降低或消除与感应带电相关的不希望效应的乳液聚集调色剂。
背景技术
对于黑色和彩色印刷物两者,已知小粒度调色剂改进印刷物的图像质量。高速黑白打印机要求调色剂颗粒可在无油熔凝器系统中以低最小定影温度(MFT)提供无光泽润饰以能够实现高速打印和同时在获得的印刷产品中达到优异的图像质量。
已知包含炭黑或其它导电颜料的调色剂易于在高电场中发生感应带电。结果是产生大量错误标志的调色剂,该调色剂在受光体上导致过多的背景,特别是采用接触双组分显影的机器时。此感应的背景具有低的转印效率并引起两个基本问题:由于转移到介质上一些背景调色剂而使图像质量差,和由于将大多数未转移的背景调色剂直接导引到废瓶中而得到过量的废调色剂。在最严格的条件下,多至约80%所消耗的总调色剂可能损失到感应背景中。
发明内容
描述了包括基本没有交联的树脂(在此也称为非交联的树脂);交联的树脂或凝胶;蜡;和导电着色剂的调色剂组合物。描述了制备调色剂的方法,该方法包括在蜡、着色剂和凝结剂存在下混合基本没有交联的树脂和交联的树脂以提供调色剂尺寸聚集体;向形成的聚集体中加入另外的基本没有交联的树脂由此在形成的聚集体上提供;加热壳覆盖的聚集体以形成调色剂;和非必要地分离调色剂。在实施方案中,加热包括在基本没有交联的树脂的玻璃化转变温度以下的第一加热和在基本没有交联的树脂的玻璃化转变温度以上的第二加热;
着色剂是存在数量为约4wt%-约18wt%的导电着色剂,基于调色剂组合物的重量;存在数量为约6wt%-约10wt%或约8wt%-约9wt%的导电着色剂,基于调色剂组合物的重量;着色剂的体积平均粒径为约50-约300纳米;着色剂是导电颜料、黑颜料或炭黑。在此使用的导电着色剂表示例如电导率为约1×10-6西门子每厘米(S/cm)-约1×104S/cm或约1×10-2S/cm-约100S/cm或约0.1S/cm-约10S/cm的着色剂。电导率由任何合适的方法例如导电材料电阻率的ASTM标准测试方法ASTM B193-02或ASTM动力电阻率测试WK5909测量。在实施方案中,调色剂组合物提供例如公称转印调色剂单位面积质量(TMA)为约0.35-约0.55mg/cm2的乳液聚集调色剂;公称TMA定义为使所得图像具有所需的颜色密度水平;例如,对于单色(黑白)图像所需的发光度水平可以为约19-约25或约20-约23;调色剂组合物提供调色剂,例如斑点等级为约25-约35,粒状斑点等级为约4-约5的乳液聚集调色剂,
公称显影电压为约200V-约300V的乳液聚集调色剂。显影电压定义为在要求产生对应公称TMA的受光体的显影剂和图像区域之间静电电势之差。在进一步的实施方案中,调色剂组合物提供例如对于单色应用受光体背景小于约60粒/mm2的乳液聚集调色剂;
在各方面提供满足复印机要求的特性如最小定影温度、宽熔凝范围、良好的脱除性能、低光泽、牢固颗粒、所需的摩擦电性能和在高速度如150ppm(即字母尺寸单侧印刷每分钟)和以上的速度下的显影;提供着色剂范围,例如导电颜料如炭黑,该着色剂例如可用于单色应用的双组分磁性刷显影以提供优异的图像质量而同时最小化或消除与感应带电相关的不希望效果。
在实施方案中,提供包括本组合物和载体的显影剂,采用本组合物制备图像的设备,例如包括充电组件、成像组件、光电导组件、显影组件、转印组件和熔凝组件的静电复印设备,其中显影组件包括本显影剂,包括高速打印机、黑白高速打印机、彩色打印机或其结合的设备。
具体实施方式
包括非交联的树脂,交联的树脂或凝胶,蜡,和着色剂的调色剂组合物具有优化的着色剂含量以提供优异的图像质量以及减轻或消除与感应带电相关的不希望效果。进一步提供调色剂方法,该方法包括在蜡、着色剂和凝结剂存在下混合非交联的树脂和交联的树脂或凝胶;其中着色剂存在的数量足以提供优异的图像质量以及减轻或消除与感应带电相关的不希望效果;向形成的聚集体中加入另外的非交联胶乳由此在形成的聚集体上提供壳;加热壳覆盖的聚集体以形成调色剂;和非必要地分离调色剂。
该方法在实施方案中提供数量为约0.01wt%-约20wt%的阴离子表面活性剂,基于反应混合物的总重量;其中阴离子表面活性剂选自十二烷基硫酸钠、十二烷基苯磺酸钠、十二烷基萘硫酸钠、二烷基苯烷基硫酸盐、磺酸盐、己二酸、十六烷基二苯基氧化物二磺酸盐或其混合物;调色剂方法,其中壳的厚度为约0.3-约0.8微米;
成像方法包括采用在此所述的调色剂组合物在受光体上显影图像。
在此使用的基本没有交联的树脂表示例如基本含有0%交联到小于约0.1%交联的树脂。在实施方案中,交联树脂或凝胶包括含有例如约0.3%-约20%交联的交联树脂或凝胶。
在实施方案中,调色剂组合物包括约68wt%-约75wt%基本没有交联的树脂、约6wt%-约13wt%交联的树脂、约6wt%-约12wt%蜡和约4wt%-约18wt%导电着色剂,基于组合物的总重量并且其中所述组分的总和是约100%;
着色剂是存在数量为约4wt%-约18wt%,或约6wt%-约10wt%,或约8wt%-约9wt%的颜料,例如导电颜料如炭黑,基于调色剂组合物的重量;
调色剂组合物提供公称转印调色剂单位面积质量(TMA)为约0.35-约0.55mg/cm2的乳液聚集调色剂;
调色剂组合物提供斑点等级为约25-约35的乳液聚集调色剂;
调色剂组合物提供粒状斑点等级为约4-约5的乳液聚集调色剂;
调色剂组合物提供公称显影电压为约200V-约300V的乳液聚集调色剂;
调色剂组合物提供受光体背景小于约60粒/mm2的乳液聚集调色剂。
选择用于非交联的树脂和交联的树脂或凝胶的胶乳树脂或聚合物的说明性例子包括已知聚合物如苯乙烯丙烯酸酯、苯乙烯甲基丙烯酸酯、丁二烯、异戊二烯、丙烯腈、丙烯酸、甲基丙烯酸、丙烯酸β-羧基乙酯、聚酯、聚(苯乙烯-丁二烯)、聚(甲基苯乙烯-丁二烯)、聚(甲基丙烯酸甲酯-丁二烯)、聚(甲基丙烯酸乙酯-丁二烯)、聚(甲基丙烯酸丙酯-丁二烯)、聚(甲基丙烯酸丁酯-丁二烯)、聚(丙烯酸甲酯-丁二烯)、聚(丙烯酸乙酯-丁二烯)、聚(丙烯酸丙酯-丁二烯)、聚(丙烯酸丁酯-丁二烯)、聚(苯乙烯-异戊二烯)、聚(甲基苯乙烯-异戊二烯)、聚(甲基丙烯酸甲酯-异戊二烯)、聚(甲基丙烯酸乙酯-异戊二烯)、聚(甲基丙烯酸丙酯-异戊二烯)、聚(甲基丙烯酸丁酯-异戊二烯)、聚(丙烯酸甲酯-异戊二烯)、聚(丙烯酸乙酯-异戊二烯)、聚(丙烯酸丙酯-异戊二烯)、聚(丙烯酸丁酯-异戊二烯)、聚(苯乙烯-丙烯酸丙酯)、聚(苯乙烯-丙烯酸丁酯)、聚(苯乙烯-丁二烯-丙烯酸)、聚(苯乙烯-丁二烯-甲基丙烯酸)、聚(苯乙烯-丙烯酸丁酯-丙烯酸)、聚(苯乙烯-丙烯酸丁酯-甲基丙烯酸)、聚(苯乙烯-丙烯酸丁酯-丙烯腈)、聚(苯乙烯-丙烯酸丁酯-丙烯腈-丙烯酸)和苯乙烯/丙烯酸丁酯/羧酸三元共聚物等或其混合物;苯乙烯/丙烯酸丁酯/羧酸三元共聚物。
例如,在实施方案中选择的树脂以各种有效数量例如调色剂的约62wt%-约83wt%存在,并且在由Brookhaven纳米尺寸颗粒分析仪测量的平均体积直径中胶乳粒度是约0.05微米-约1微米。可以在实施方案中选择胶乳颗粒的其它尺寸和有效量。
在实施方案中,选择的胶乳树脂由乳液聚合方法制备,并且单体包括例如苯乙烯、丙烯酸酯、甲基丙烯酸酯、丁二烯、异戊二烯、丙烯腈、丙烯酸和甲基丙烯酸,尽管不是限制性的。已知的链转移剂,例如有效量为例如约0.1-约10%的十二烷硫醇,和/或有效量为约0.1-约10%的四溴化碳也可用于控制聚合期间的树脂分子量。获得例如约0.05微米-约1微米的树脂颗粒的其它方法可以选自聚合物微悬浮方法,如在美国专利3,674,736中公开的方法,聚合物溶液微悬浮方法,如在美国专利5,290,654中公开的方法,或其它已知方法。
在实施方案中,非交联的树脂和交联的树脂或凝胶的至少一种包括数量为约0.05-约10wt%的羧酸,基于非交联的树脂或交联的树脂或凝胶的总重量。
在实施方案中数量例如为反应混合物的约0.01-约20wt%,或约0.1-约15wt%的表面活性剂包括例如非离子表面活性剂如购自Rhone-Poulenc的二烷基苯氧基聚(乙烯氧)乙醇。在实施方案中非离子表面活性剂的有效浓度是例如反应混合物的约0.01-约10wt%,或约0.1-约5wt%。
阴离子表面活性剂的例子包括例如十二烷基硫酸钠(SDS)、十二烷基苯磺酸钠、十二烷基萘硫酸钠、二烷基苯烷基硫酸盐和磺酸盐、己二酸等。通常采用的阴离子表面活性剂的有效浓度是例如反应混合物的约0.01-约10wt%,或约0.1-约5wt%。
用于增加pH和因此电离聚集体颗粒并由此提供稳定性和防止聚集体尺寸增加的碱的例子选自氢氧化钠、氢氧化钾、氢氧化铵、氢氧化铯等。
可以在聚结之前或期间非必要地随增加的温度加入聚集体悬浮液以例如防止聚集体尺寸增加或稳定聚集体尺寸的另外的表面活性剂的例子可以选自阴离子表面活性剂如十二烷基苯磺酸钠、十二烷基萘硫酸钠、二烷基苯烷基硫酸盐和磺酸盐、己二酸等。这些表面活性剂也可以选自非离子表面活性剂如聚乙烯醇、聚丙烯酸、methalose、甲基纤维素、乙基纤维素、丙基纤维素、羟乙基纤维素、羧甲基纤维素、聚氧乙烯鲸蜡基醚、聚氧乙烯月桂基醚、聚氧乙烯辛基醚、聚氧乙烯辛基苯基醚、聚氧乙烯油基醚、聚氧乙烯脱水山梨醇单月桂酸酯、聚氧乙烯硬脂醚、聚氧乙烯壬基苯基醚、二烷基苯氧基聚(乙烯氧)乙醇。通常用作聚集体尺寸稳定剂的阴离子或非离子表面活性剂的有效量是例如反应混合物的约0.01wt%-约10wt%或约0.1wt%-约5wt%。
可以采用的酸的例子包括例如硝酸、硫酸、盐酸、乙酸、柠檬酸、三氟乙酸、琥珀酸、水杨酸等,并且该酸在实施方案中以水的约0.5-约10wt%或水的约0.7-约5wt%的稀释形式采用。
例如,适于本调色剂组合物的蜡包括但不限于具有约1-约25个碳原子的亚烷基蜡,包括例如聚乙烯、聚丙烯或其混合物。蜡的例子包括在此说明的那些,如上述共同未决申请的那些,购自AlliedChemical and Petrolite Corporation的聚丙烯和聚乙烯,购自Michaelman Inc.and Daniels Products Company的蜡乳液,购自Eastman Chemical Products,Inc.的Epolene N-15TM、Viscol 550-PTM,购自Sanyo Kasei K.K.的低重均分子量的聚丙烯和相似材料。相信市售的聚乙烯的分子量(Mw)为1,000-约5,000,并相信市售聚丙烯的分子量为约4,000-约10,000。官能化蜡的例子包括胺、酰胺、氟化蜡、混合的氟化酰胺蜡、酰亚胺、酯、季胺、羧酸或丙烯酸类聚合物乳液、氯化聚丙烯和聚乙烯。
在实施方案中,蜡包括分散体形式的蜡,该分散体包括体积平均粒径为约100纳米-约500纳米的蜡、水和阴离子表面活性剂。蜡的含量是例如约3-约30wt%或约5-约15wt%,基于组合物的总重量。在实施方案中,蜡包括聚乙烯蜡颗粒,尽管公开内容不限于此,粒径为约100-约500纳米。在实施方案中用于分散蜡的表面活性剂是阴离子表面活性剂,尽管不限于此。
适于本调色剂方法的导电着色剂或颜料的例子包括但不限于颜料、染料、颜料和染料的混合物、颜料混合物、染料混合物等。导电着色剂可具有例如黑色(如炭黑)、青色、黄色、品红色、蓝色、或其混合的颜色。在实施方案中,导电着色剂包括颜料、染料、炭黑、磁铁矿、黑着色剂、青着色剂、品红色着色剂、黄色着色剂、红色着色剂、绿色着色剂、蓝色着色剂、棕色着色剂、其混合物,数量例如为约1%-约25wt%,基于组合物的总重量,其中组分的总和是约100%。
可以使用的导电着色剂的例子包括但不限于磁铁矿和表面处理的磁铁矿。可以使用的合适黑颜料是例如炭黑如REGAL 330TM等。作为有色颜料,可以选择青色、品红色、黄色、红色、绿色、棕色、蓝色或其混合的颜料。着色剂也可以由预分散的颜料组成如是市购的。示例颜料分散体包括来自Sun Chemical的FLEXIVERSE系列和SUNSPERSE系列颜料分散体。
例如,在实施方案中,着色剂包括黑颜料。在另外的实施方案中,着色剂包括炭黑。在另外的实施方案中,颜料包括形状因子为约120-约140、圆形度为约0.900-约0.980的黑调色剂颗粒,或其组合。
另外的有用着色剂包括在水基分散体中的颜料如购自SunChemical的那些等或其混合物。
用于本方法的凝结剂包括聚金属卤化物,如聚氯化铝(PAC)或聚磺基硅酸铝(PASS)。凝结剂提供金属含量为例如约400-约10,000份每百万份的最终调色剂。在另一个特征中,凝结剂包括聚氯化铝,提供铝含量为约400-约10,000份每百万份的最终调色剂。
包括在此称为单体A、B和C的苯乙烯、丙烯酸丁酯和丙烯酸β-羧基乙酯(β-CEA)单体的非交联胶乳是例如在引发剂、链转移剂(CTA)和表面活性剂存在下由乳液聚合制备的。例如,各单体的组组在实施方案中是约70%-约90%苯乙烯,约73%-约85%苯乙烯,或约76.5%苯乙烯,约10%-约30%丙烯酸丁酯,约15%-约27%丙烯酸丁酯,或约23.5%丙烯酸丁酯,和约0.5%-约10%β-CEA,约1.0%-约5%β-CEA,或约3%β-CEA,尽管不限于这些特定类型的单体或范围。
引发剂可以是例如但不限于过硫酸钠或过硫酸铵,并且存在的范围为约0.5-约3.0%,基于单体的重量,尽管不是限制性的。CTA存在的数量例如为约1.5-约3.0wt%,基于单体A和B的组合重量,尽管不是限制性的。表面活性剂例如是存在范围为约0.7-约5.0wt%的阴离子表面活性剂,基于水相的重量,尽管不限于此类型或范围。
例如,在如美国专利5,444,140和5,455,315提及的贫进料条件下聚合单体,以提供尺寸为约100-约300纳米的胶乳树脂颗粒。胶乳树脂的分子量是约30,000-约37,000,尽管不限于此范围。开始玻璃化转变温度(TG)不受限制但可以为例如约46℃-约60℃或约51℃。在实施方案中,羧酸基团的数量是约0.05-约4.0份每百份树脂单体A和B。获得的聚合物树脂的开始Tg是约51℃,尽管不限于此,分子量(Mw)是约30,000-约37,000或约34,000,分子数(Mn)是约5,000-约20,000或约11,000,尽管不限于此,以提供pH为约1.0-约4.0或约2.0的非交联胶乳。
例如,交联胶乳是在引发剂如过硫酸盐、CTA和表面活性剂存在下由乳液聚合从包括在此称为单体A、B、C和D的苯乙烯、丙烯酸丁酯、β-CEA和二乙烯基苯的非交联胶乳制备的。在实施方案中单体组成包括约60%-约75%苯乙烯或约65%苯乙烯,约25%-约40%丙烯酸丁酯或约35%丙烯酸丁酯,约3%-约5%β-CEA或约3%β-CEA,和约3%-约5%二乙烯基苯或约1%二乙烯基苯,尽管组成不限于这些数量。交联胶乳的Tg(开始)是约40℃-约55℃或约42℃且交联程度是约0.3-约20%,尽管不限于此,这是由于二乙烯基苯浓度的增加会增加交联。在实施方案中交联胶乳的可溶性部分的Mw为约135,000而Mn为约27,000,但不限于此。交联胶乳的粒度是约50纳米,尽管不是限制性的,并且可以为约20-约250纳米。表面活性剂可以是任何表面活性剂,例如但不限于阴离子表面活性剂如Neogen RK或TAYCAPOWDER BN 2060。胶乳的pH是约1.5-约3.0或约1.8。
在实施方案中,蜡为分散体形式,该分散体包括粒径为约100纳米-约500纳米的蜡、水和阴离子表面活性剂。例如,制备蜡分散体,其中蜡在实施方案中包括聚乙烯蜡颗粒,如购自Baker Petrolite的Polywax 850,尽管不限于此,粒径为约100-约500纳米,尽管不是限制性的。在各方面,用于分散蜡的表面活性剂是阴离子表面活性剂,尽管不限于此,例如购自Tayca Corporation的TAYCAPOWER BN 2060。
在实施方案中,着色剂包括颜料分散体,该分散体包括体积平均粒径为约50-约300纳米的颜料颗粒、水和阴离子表面活性剂。例如,如在阴离子表面活性剂中采用市售的Regal 330TM和非必要的非离子分散体制备炭黑以提供尺寸为约50纳米-约300纳米的颜料颗粒。用于分散炭黑的表面活性剂在实施方案中是阴离子表面活性剂如Neogen RKTM或Taycapowder,尽管不限于此。Ultimizer型设备用于提供颜料分散体,尽管也可以使用介质磨或其它装置。
在实施方案中,调色剂方法包括在蜡和颜料分散体存在下混合非交联胶乳与一定数量的交联胶乳,向颜料分散体中加入聚金属卤化物如聚氯化铝的凝结剂,同时在高速下如用polytron共混,形成调色剂颗粒。通过加热到低于树脂Tg的温度聚集pH为约2.0-约3.0的所得混合物以提供调色剂尺寸聚集体。向形成的聚集体中加入另外的非交联胶乳,在形成的聚集体上提供壳。然后通过加入氢氧化钠溶液改变混合物的pH直到达到约7.0的pH。当混合物达到约7.0的pH时,羧酸电离以在聚集体上提供另外的负电荷,由此提供稳定性并防止颗粒进一步生长或当在胶乳树脂的Tg以上加热时尺寸分布的增加。然后将混合物的温度升高到约95℃。在约30分钟之后,将混合物的pH降低到当进一步加热时足以聚结或熔凝聚集体以提供复合颗粒的数值,如约4.5。例如采用Sysmex FPIA 2100分析仪测量熔凝颗粒的形状因子或圆形度,直到达到需要的形状。
允许混合物冷却到室温并洗涤该混合物。例如在约10的pH和约63℃的温度下进行第一次洗涤,随后在室温下进行去离子水(DIW)洗涤。在此之后在约4.0的pH和约40℃的温度下洗涤,随后进行最后的DIW水洗涤。然后干燥调色剂。
在包括非交联胶乳、交联胶乳、蜡和颜料的本调色剂组合物中,交联的胶乳主要用于增加热污损(offset),而蜡用于提供剥离特性。选择非交联胶乳与交联胶乳的比例、蜡含量与着色剂含量的比例以控制调色剂的流变。在实施方案中,调色剂包括约62%-约82%的非交联树脂,约6%-约13%的交联树脂或凝胶,约6%-约12%的蜡,和约6%-约13%的着色剂,或约71wt%的非交联树脂,约10wt%的交联树脂,约9wt%的蜡,和约10wt%的颜料,基于组合物的总重量。在另外的实施方案中,调色剂包括约120-约140的形状因子(形状因子=100×最大直径2/(面积×π/4));约0.900-约0.980的颗粒圆形度;复合调色剂颗粒的分子量为约25,000-约40,000或约35,000,分子数为约9,000-约13,000或约10,000,且开始Tg为约48℃-约62℃或约54℃;非交联的树脂包括约76.5wt%苯乙烯、约23.5wt%丙烯酸丁酯和约3.0wt%β-CEA,基于非交联树脂的总重量并且交联胶乳包括约65wt%苯乙烯、约35wt%丙烯酸丁酯、约3wt%β-CEA和约1.0wt%二乙烯基苯,基于交联树脂的总重量。
例如,称为EP5的胶乳乳液如下制备,该乳液包括从苯乙烯,丙烯酸正丁酯和β-CEA的乳液聚合产生的聚合物颗粒。通过在不锈钢储存罐中混合约10分钟制备由约605克DowfaxTM 2A1阴离子乳化剂和约387kg去离子水组成的表面活性剂溶液。然后在转移入反应器之前采用氮气吹扫储存罐约5分钟。然后将反应器采继续用氮气吹扫同时在约100rpm下搅拌。然后将反应器在受控速率下加热到约75℃并在约75℃下保持整个反应直到冷却或是对于反应主要部分为约6-约7小时。单独地,将约6.1kg过硫酸铵引发剂溶于约30.2kg去离子水。如下单独制备单体乳液。将约311.4kg苯乙烯、约95.6kg丙烯酸丁酯、约12.21kgβ-CEA、约2.88kg 1-十二烷硫醇、约1.42kgADOD、约8.04kg Dowfax 2A1TM阴离子表面活性剂和约193kg去离子水混合以形成乳液。然后在约75℃下将约1%形成的乳液缓慢加入包含表面活性剂水相的反应器中以形成晶种同时采用氮气吹扫。然后将引发剂溶液缓慢加入到反应器中。在约20分钟之后,使用计量泵以约0.5毫升/分钟的速率连续向反应器中加入剩余的乳液。一旦将所有的单体乳液加入到主反应器中,将温度保持在约75℃下另外3小时以完成反应。然后进行完全冷却并将反应器温度降低到约35℃。将获得的产物收集入储存罐并随后干燥。在干燥之后胶乳的分子性能如下:Mw=35,419;Mn=11,354;开始Tg=51.0℃。
例如,如下制备称为EA15-8的胶乳乳液,该乳液包括从苯乙烯、丙烯酸正丁酯、二乙烯基苯和β-CEA的半连续乳液聚合产生的聚合物凝胶颗粒。通过在不锈钢储存罐中混合约10分钟制备由约1.75千克Neogen RKTM阴离子乳化剂和约145.8千克去离子水组成的表面活性剂溶液。然后在转移入反应器之前采用氮气吹扫储存罐约5分钟。然后继续用氮气吹扫反应器同时在约300rpm下搅拌。然后将反应器在受控速率下加热到约75℃的温度并保持恒定。在单独的容器中,将约1.24千克过硫酸铵引发剂溶于约13.12千克去离子水中。在第二个单独的容器中,如下制备单体乳液。将约47.39千克苯乙烯、约25.52千克丙烯酸正丁酯、约2.19千克β-CEA、约729克55%等级二乙烯基苯、约4.08千克Neogen RKTM阴离子表面活性剂和约78.73千克去离子水混合物以形成乳液。苯乙烯单体与丙烯酸正丁酯单体的比例是约65-约35wt%。在约75℃下在氮气吹扫下将约1%形成的乳液缓慢加入到包含表面活性剂水相的反应器以形成晶种。然后将引发剂溶液缓慢加入到反应器中并静置约20分钟。在约20分钟静置之后,使用计量泵将剩余的乳液连续加入反应器。一旦将所有的单体乳液加入主反应器,将温度保持在约75℃下另外4小时以完成反应。然后进行完全冷却并将反应器温度降低到约35℃。在通过1微米过滤垫过滤之后将产物收集入储存罐中。在干燥一部分胶乳之后,分子性能测量如下:Mw=134,700;Mn=27,300;开始Tg=43℃。采用盘式离心机测量的胶乳的平均粒度是约48纳米。由气相色谱测量的残余单体对于苯乙烯小于约50份每百万份而对于丙烯酸正丁酯小于约100份每百万份。
将约191.4克固体含量为约41.4wt%的EP5胶乳和约55.22克固体含量为约30.07wt%的EAWax-91蜡乳液(Polywax 850)加入在容器中的约478.6克去离子水中并采用在约4,000rpm下操作的IKAUltra TurraxT50均化器搅拌。其后,将约113.51克固体含量为约17wt%的黑颜料分散体Sun Pigment WA 1945(Regal 330)、约75克固体含量为24wt%的EA15-8胶乳凝胶和约9.91克1wt%氯化钙溶液加入到上述混合物中,然后滴加约30.6克包含约3.06克聚氯化铝混合物和约27.54克0.02摩尔浓度(M)硝酸溶液的絮状混合物。在滴加絮状混合物时,将均化器速度增加到约5,200rpm并均化另外5分钟。其后,将混合物以1℃每分钟加热升温到约49℃并保持约1.5-约2小时,得到由库乐尔特粒度计测量的体积平均粒径为约5微米。在加热期间,搅拌器在约250rpm下运行。在达到49℃的设定温度之后约10分钟,将搅拌器速度降低到约220rpm。将另外124.6克EP5胶乳加入到反应器混合物中并在约49℃下聚集另外约30分钟,得到约5.7微米的体积平均粒径。采用1.0M氢氧化钠溶液将反应器混合物的pH调节到约7。然后将反应器混合物以约1℃每分钟加热升温到约95℃。然后采用0.3M硝酸溶液将混合物的pH调节到约3.7。将反应器混合物在约95℃下轻微搅拌约5小时以聚结和球形化颗粒。然后关闭反应器加热器并使混合物以约1℃每分钟的速率冷却到室温。获得的调色剂混合物由约16.7wt%调色剂、约0.25wt%阴离子表面活性剂和约82.9wt%水组成。此混合物的调色剂包括约71wt%苯乙烯/丙烯酸酯非交联聚合物、约10wt%EA15-8凝胶、约10wt%Regal 330颜料、约9wt%PW850蜡、约150份每百万份氯化钙,并且体积平均粒径为约5.7微米,GSD为约1.19。洗涤颗粒6次,第一次洗涤在约10的pH和约63℃下进行,随后采用去离子水在室温下进行3次洗涤,随后在约4.0的pH和约40℃下洗涤一次,并采用去离子水在室温下进行最后的洗涤。
在实施方案中,通过使用例如约2%调色剂浓度到约8%调色剂浓度混合采用本方法获得的调色剂与已知载体颗粒制备显影剂组合物,所述载体颗粒包括涂覆的载体,如钢、铁氧体等;也可包含在聚合物涂料中分散的导电化合物,如导电炭黑并且该导电化合物以各种合适的数量,如约15-约65wt%,或约20-约45wt%存在;提供显影剂方法,该方法包括制备显影剂,该显影剂包括在此在实施方案中公开的组合物和载体;制备图像的方法包括在图像形成设备中采用本组合物;制备图像的方法包括在图像形成设备中采用本组合物,该设备包括高速打印机、黑白高速打印机、或其结合;调色剂,优选乳液聚集调色剂包括非交联的树脂、交联的树脂或凝胶、蜡和导电着色剂,其中导电着色剂存在的数量为约4wt%-约18wt%,或约6wt%-约10wt%,或约8wt%-约9wt%,基于调色剂组合物的重量;调色剂的公称转印调色剂单位面积质量(TMA)为约0.35-约0.55mg/cm2;调色剂的斑点等级为约25-约35;调色剂的粒状斑点等级为约4-约5;调色剂的公称显影电压为约200V-约300V;调色剂的受光体背景小于约60粒/mm2;
导电颜料存在的数量为约6wt%-约10wt%,或约8wt%-约9wt%,并且提供优异的图像质量并同时降低或消除不希望的带电效果。尽管不希望受理论约束,但范围的下限与在公称TMA下提供优异的图像质量有关;即为成本效率而最小化公称TMA,而范围的上限与感应带电效果以及与摩擦电电荷中不希望的降低相关。
在实施方案中,调色剂组合物的分子量为约25,000-约40,000。此外,调色剂组合物在实施方案中的分子数为约9,000-约13,000。
根据以上描述的过程制备如下实施例以举例说明包括优化颜料含量的各方面。基础颗粒包括重量比为约76.5%苯乙烯、23.5%丙烯酸丁酯和约3%β-CEA的苯乙烯:丙烯酸丁酯:β-CEA,10%交联凝胶胶乳,9%PW850蜡,0.17pph聚氯化铝(PAC)聚集剂和约6-约10%炭黑颜料,如表1所列。
表1
实施例# | 1 | 2 | 3 | 4 | 5 | 6 | 7 | |
胶乳 | SDC-EP28乳液聚合胶乳 | |||||||
凝胶胶乳 | EA15-8 | |||||||
颜料 | 分散体 | Sun分散体WA1945 | Cavitron分散体PD-K7 | |||||
含量 | 6% | 8% | 10% | 6% | 8% | 9% | 10% | |
粒度 | D50 | 5.77 | 5.64 | 5.62 | 5.71 | 5.72 | 5.75 | 5.59 |
GSDv | 1.19 | 1.19 | 1.19 | 1.19 | 1.19 | 1.20 | 1.19 | |
GSDn | 1.23 | 1.22 | 1.22 | 1.23 | 1.22 | 1.23 | 1.23 |
在表1中,SDC-EP28表示由SDC提供的乳液聚合胶乳批号SDC-DP28,EA15-8表示以上所述的凝胶胶乳批号(由乳液聚合的交联胶乳制备),Sun分散体WA1945表示来自SUN Chemical的炭黑分散体批号,Cavitron分散体PD-K7表示购自XRCC的炭黑分散体批号PD-K7。D50表示平均粒度,GSDv表示体积几何标准偏差,GSDn表示数目几何标准偏差。
采用在实施例1-7中描述的每种调色剂制备显影剂包(package),包括粉末涂覆的载体和表面添加剂包,所述载体包括35微米球形镁-锶铁氧体磁心(Powdertech Corp.,日本),所述表面添加剂包包括约1.71%疏水性50纳米煅烧的二氧化硅、约0.74%120纳米疏水性溶胶-凝胶二氧化硅和约0.37%疏水性40纳米二氧化钛。
将约400克载体和约24克调色剂的混合物放入Xerox DC12打印机的显影剂外壳内。通过吹掉未熔凝的调色剂和将含有和不含有调色剂的衬底称重测量TMA。在电荷光谱仪中通过目视测量从零场点位置调色剂偏离的上下限测量q/d。在粘合带上收集在受光体上的背景,并使用实验室光学显微镜计数每mm2的颗粒数目。
采用DC12打印机在Xerox 4024纸衬底上制备尺寸为1英寸×2英寸的未熔凝实心区域和半色图像。将这些图像在Xerox DT120熔凝器中熔凝。将加工速度设定为829mm/s并使尖端宽度保持在13.5mm。采用设定到185℃的辊温度熔凝所有的样品。
Xerox Corporation IQAF(Xerox Corporation专用图像质量分析包)用于测量实心区域密度、斑点和粒度。图像质量结果归纳在表2中。
表2
分散体类型 | 目标 | Sun | Cavitron | CB含量范围 | |||||
CB% | 6 | 8 | 10 | 6 | 8 | 9 | 10 | ||
q/d,fC/μm(A-区,60min漆-震动) | <-0.2 | -0.40 | -0.32 | -0.29 | -0.34 | -0.26 | -0.32 | 目标满足所有CB含量 | |
Q/d,fC/μm(C-区,60min漆-震动) | <-0.2 | -1.26 | -1.02 | -0.99 | -1.32 | -0.94 | -0.89 | 目标满足所有CB含量 | |
在TMA=0.4mg/cm2的斑点(最大值) | 40 | ND | ND | ND | 25 | 35 | 30 | 30 | 目标在公称TA满足所有CB含量 |
在TMA=0.4mg/cm2下的粒度(最大值) | 5 | ND | ND | ND | 4.1 | 4.8 | 5.0 | 5.1 | 要求<10%以满足目标 |
显影电压,V | <300 | 450 | 230 | 250 | 320 | 225 | 280 | 270 | 要求>6%以满足目标 |
受光体背景,粒/mm2 | <60 | <15 | 37 | 65 | 10 | 38 | 56 | 72 | 要求<10%以满足目标 |
废瓶填充率(DC555),g/千印 | <8 | ND | 1 | 14 | ND | ND | ND | ND | 要求<10%以满足目标 |
在表2中,使用以上电荷光谱方法评价以飞姆托-库仑每微米计的q/d,A区=85%RH和28℃,而C区=15%RH和10℃。
所有的调色剂具有非常相似的充电特性。q/d变化的范围是-1.32到-0.26,然而甚至在炭黑(CB)着色剂的最高含量下也在-0.2fC/微米的目标值以下。斑点低,在约25-约35范围(可见斑点是40-50和更高)。受光体背景随CB含量增加(由于电感应);然而在最高达约10%CB时仍保持在<60粒/mm2的范围。因此,约6-约9%的CB含量范围已足够低可以防止摩擦电电荷中的不希望的降低和不希望的感应背景,并且对于良好图像质量是足够高的。
Claims (4)
1.一种调色剂组合物,包括:
基本没有交联的树脂;
交联的树脂;
蜡;和
导电着色剂。
2.权利要求1的调色剂组合物,其中导电着色剂存在的数量为约4wt%-约18wt%,基于调色剂组合物的总重量,并且其中组分的总和是约100%。
3.权利要求1的调色剂组合物,其中导电着色剂的体积平均粒径为约50-约300纳米。
4.权利要求1的调色剂组合物,其中导电着色剂包括存在数量为约6wt%-约10wt%的炭黑,基于调色剂组合物的总重量,并且其中组分的总和是约100%。
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-
2004
- 2004-12-03 US US11/003,297 patent/US20060121380A1/en not_active Abandoned
-
2005
- 2005-12-02 CN CN200510128939.7A patent/CN1782891A/zh active Pending
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101315527B (zh) * | 2007-05-31 | 2013-09-25 | 施乐公司 | 调色剂组合物的制备方法 |
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